Microspheres and microcapsules, a survey of manufacturing techniques: Part III: Solvent evaporation

A methodological survey of microsphere formation and microencapsulation techniques based on solvent extraction/evaporation techniques is presented. Thus, basic features of solvent extraction and solvent evaporation processes, including droplet formation, droplet/particle stabilization, and solvent removal, are outlined. Preparation of a wide range of microspherical and microcapsular products based on biodegradable polyesters, polysaccharides, and nonbiodegradable polymers are discussed. Dependence of microcapsule characteristics on manufacturing parameters, as well as performance evaluation of microspherical and microcapsular products, are also briefly covered.

Syntheses of opened hollow clay microspheres through a spray-drying approach and their derivative clay/carbon nanotubes composites

Opened hollow microspheres of organoclays were prepared via spray drying the suspension of modified Na+-montmorillonite (Na+-MMT) with alkylsulfonate. The microstructure and thermal properties of these opened hollow spheres were characterized by means of wide-angle X-ray diffraction, field emission scanning electron microscopy, and thermogravimetric analysis. The results showed that the organoclays had larger interlayer spacing compared with pure Na+-MMT and higher thermal stability relative to the alkylsufonate.

Energy transfer and tunable luminescence properties of Eu3+ in TbBO3 microspheres via a facile hydrothermal process

Tb(1-x)BO3:xEu(3+) (x = 0-1) microsphere phosphors have been successfully prepared by a simple hydrothermal process directly without further sintering treatment. X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), thermogravimetric analysis (TGA), scanning electron microscopy (SEM), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), selected area electron diffraction (SAED), photoluminescence (PL), low-voltage cathodoluminescence (CL), and time-resolved emission spectra as well as lifetimes were used to characterize the samples.

Grafting BSA onto poly[(L-lactide)-co-carbonate] microspheres by click chemistry

Model protein bovine serum albumin (BSA) was covalently grafted onto poly[(L-lactide)co-carbonate] microsphere surfaces by "click chemistry." The grafting was confirmed by confocal laser scanning microscopy and X-ray photoelectron spectroscopy. The maximum amount of surface-grafted BSA was 45 mg.g(-1). The secondary structure of the grafted BSA was analyzed by FTIR and the results demonstrated that the grafting did not affect protein structure. This strategy can also be used on microspheres prepared from poly(L-lactide)/poly[(L-lactide)-co-carbonate] blend materials.

3D Fe3S4 flower-like microspheres: high-yield synthesis via a biomolecule-assisted solution approach, their electrical, magnetic and electrochemical hydrogen storage properties

Well-defined 3D Fe3S4 flower-like microspheres were synthesized via a simple biomolecule-assisted hydrothermal process for the first time. On the basis of a series of contrast experiments, the probable growth mechanism and fabrication process of the products were proposed. The electrical conductivity property of the as-synthesized Fe3S4 sample exhibited a rectifying characteristic when a forward bias was applied for the bottom-contacted device. The magnetic properties of the products were studied as well and the results demonstrated that the products presented ferromagnetic properties related to the corresponding microstructure. In addition, we first verified that the Fe3S4 flower-like microspheres could store hydrogen electrochemically, and a discharge capacity of 214 mA h g(-1) was measured without any activation under normal atmospheric conditions at room temperature.

Insulin nanoparticle preparation and encapsulation into poly(lactic-co-glycolic acid) microspheres by using an anhydrous system

Insulin has been encapsulated in poly(lactic-co-glycolic acid) (PLGA) microspheres by solid-in-oil-in-oil (S/O/O) emulsion technique using DMF/corn oil as new solvent pairs. To get better encapsulation efficiency, insulin nanoparticles were prepared by the modified isoelectric point precipitation method so that it had good dispersion in the inner oil phase. The resulting microspheres had drug loading of 10% (w/w), while the encapsulation efficiency could be up to 90-100%. And the insulin release from the microspheres could last for 60 days. Microspheres encapsulated original insulin with the same method had lower encapsulation efficiency, and shorter release period. Laser scanning confocal microscopy indicated the insulin nanoparticle and original insulin had different distribution in microspheres. The results suggested that using insulin nanoparticle was better than original insulin for microsphere preparation by S/O/O method.

Architectures of Strontium Hydroxyapatite Microspheres: Solvothermal Synthesis and Luminescence Properties

Strontium hydroxyapatite (Sr-5(PO4)(3)OH, SrHAp) microspheres with 3D architectures have been successfully prepared through a efficient and facile solvothermal process. The experimental results indicate that the SrHAP microspheres are composed of a large amount of nanosheets, which are assembled in a radial form from the center to the surface of the microspheres. The as-obtained SrHAp samples show an intense and bright blue emission from 350 to 570 nm centered at 427 nm (CIE coordinates: x = 0.153, y = 0.081; lifetime: 9.2 ns; quantum efficiency: 31%) under long-wavelength UV light excitation (344 nm). This blue emission might result from the CO2 center dot- radical impurities in the crystal lattice. Furthermore, the surfactants CTAB and trisodium citrate have an obvious impact on the morphologies and the luminescence properties of the products, respectively.

Facile Synthesis and Luminescence Properties of Highly Uniform MF/YVO4:Ln(3+) (Ln = Eu, Dy, and Sm) Composite Microspheres

Uniform MF/YVO4:Ln(3+) (Ln = Eu, Dy, and Sm) composite microspheres have been prepared via a simple and economical wet-chemical route at ambient pressure and low temperature. Monodisperse micrometer-sized melamine formaldehyde (MF) colloidal particles were first fabricated by a condensation process of melamine with formaldehyde. Subsequently, well-dispersed YVO4 nanoparticles were successfully grown onto the MF microspheres to form core-shell structured composite particles in aqueous Solution. The as-obtained composite microspheres with perfect spherical shape are uniform in size and distribution, and the thickness and roughness of the YVO4 shells on MF cores could be tuned by varying the reaction temperature. The MF/YVO4:Ln(3+) composite phosphors show strong light emissions with different colors coming from different activator ions under ultraviolet excitation, which might find potential applications in fields such as light phosphor powders and advanced flat panel displays.

General and Facile Method To Prepare Uniform Y2O3:Eu Hollow Microspheres

Well-shaped Y2O3:Eu hollow microspheres have been successfully prepared on a large scale via a urea-based homogeneous precipitation technique in the presence of colloidal carbon spheres as hard templates followed by a subsequent heat treatment process. XRD results demonstrate that all the diffraction peaks of the samples can be well indexed to the pure cubic phase Of Y2O3. TEM and SEM images indicate that the shell of the uniform hollow spheres, whose diameters are about 250 nm, is composed of many uniform nanoparticles with diameters of about 20 nm, basically consistent with the estimation of XRD results. Furthermore, the main process in this method was carried out in aqueous condition, without the use of organic solvents or etching agents. The as-prepared hollow Y2O3:Eu microspheres show a strong red emission corresponding to the D-5(0)-F-7(2) transition of the Eu3+ ions under ultraviolet or low voltage excitation, which might find potential applications in fields such as light phosphor powders, advanced flat panel displays, field emission display devices, and biological labeling.

Y2O3 : Eu3+ microspheres: Solvothermal synthesis and luminescence properties

Y2O3 : Eu3+ microspheres, with an average diameter of 3 mu m, were successfully prepared through a large-scale and facile solvothermal method followed by a subsequent heat treatment. X-ray diffraction, Fourier transform infrared spectroscopy, energy-dispersive X-ray spectra, thermogravimetric and differential thermal analysis, inductive coupled plasma atomic absorption spectrometric analysis, scanning electron microscopy, transmission electron microscopy, photoluminescence spectra, as well kinetic decays, and cathodoluminescence spectra were used to characterize the samples. These microspheres were actually composed of randomly aggregated nanoparticles. The formation mechanisms for the Y2O3 : Eu3+ microspheres have been proposed on an isotropic growth mechanism. The Y2O3 : Eu3+ microspheres show a strong red emission corresponding to D-5(0) -> F-7(2) transition (610 nm) of Eu3+ under ultraviolet excitation (259 nm) and low-voltage electron beams excitation (1-5 kV), which have potential applications in fluorescent lamps and field emission displays.

Preparation of nano-hydroxyapatite/poly(L-lactide) biocomposite microspheres

Nano-hydroxyapatite (HA)/poly(L-lactide) (PLLA) composite microspheres with relatively uniform size distribution were prepared by a solid-in-oil-in-water (s/o/w) emusion solvent evaporation method. The encapsulation of the HA nanopaticles in microshperes was significantly improved by grafting PLLA on the surface of the HA nanoparticles (p-HA) during emulsion process. This procedure gave a possibility to obtain p-HA/PLLA composite microspheres with uniform morphology and the encapsulated p-HA nanoparticle loading reached up to 40 wt% (33 wt% of pure HA) in the p-HA/PLLA composite microspheres. The microstructure of composite microspheres from core-shell to single phase changed with the variation of p-HA to PLLA ratios. p-HA/PLLA composite microspheres with the diameter range of 2-3 mu m were obtained. The entrapment efficiency of p-HA in microspheres could high up to 90 wt% and that of HA was only 13 wt%. Surface and bulk characterizations of the composite microspheres were performed by measurements such as wide angle X-ray diffraction (WAXD), thermal gravimetric analysis (TGA), environmental scanning electron microscope (ESEM) and transmission electron microscopy (TEM).

Synthesis and morphology of polyethylene chains grafted onto the surface of crosslinked polystyrene microspheres

The bifunctional comonomer 4-(3-butenyl) styrene was used to synthesize crosslinked polystyrene microspheres (c-PS) with pendant butenyl groups on their surface via suspension copolymerization. Polyethylene chains were grafted onto the surface of c-PS microspheres (PS-g-PE) via ethylene copolymerizing with the pendant butenyl group on the surface of the c-PS microspheres under the catalysis of metallocene catalyst. The composition and morphology of the PS-g-PE microspheres were characterized by means of Fourier transform infrared spectroscopy, Fourier transform Raman spectroscopy, X-ray photoelectron spectroscopy, and field-emission scanning electron microscopy. It is possible to control the content of PE grafted onto the surface of c-PS microspheres by varying the polymerization time or the initial quantity of pendant butenyl group on the surface of c-PS microspheres. Investigation on the morphology and crystallization behavior of grafted PE chains showed that different surface patterns could be formed under various crystallization conditions. Moreover, the crystallization temperature of PE chains grafted on the surface of c-PS microspheres was 6 degrees C higher than that of pure PE. The c-PS microspheres decorated by PE chains had a better compatibility with PE matrix.

ZnO-based hollow microspheres: Biopolymer-assisted assemblies from ZnO nanorods

Many efforts have been made in fabricating three-dimensional (3D) ordered zinc oxide (ZnO) nanostructures due to their growing applications in separations, sensors, catalysis, bioscience, and photonics. Here, we developed a new synthetic route to 3D ZnO-based hollow microspheres by a facile solution-based method through a water-soluble biopolymer (sodium alginate) assisted assembly from ZnO nanorods. The products were characterized by X-ray diffraction, field emission scanning electron microscopy, transmission electron microscopy, selected area electron diffraction, and X-ray photoelectron spectroscopy. Raman and photoluminescence spectra of the ZnO-based hollow microspheres were obtained at room temperature to investigate their optical properties. The hollow microspheres exhibit exciting emission features with a wide band covering nearly all the visible region. The calculated CIE (Commission Internationale d'Eclairage) coordinates are 0.24 and 0.31, which fall at the edge of the white region (the 1931 CIE diagram). A possible growth mechanism of the 3D ZnO superstructures based on typical biopolymer-crystal interactions in aqueous solution is tentatively proposed, which might be really interesting because of the participation of the biopolymer.

Complex aggregates of silica microspheres by the use of a polymer template

Evaporation of a droplet of silica microsphere suspension on a polystyrene and poly(methyl methacrylate) blend film with isolated holes in its surface has been exploited as a means of particles self-assembly. During the retraction of the contact line of the droplet, spontaneous dewetting combined with the strong capillary force pack the silica microspheres into the holes in the polymer surface. Complex aggregates of colloids are formed after being exposed to acetone vapor. The morphology evolution of the underlying polymer film by exposure to acetone solvent vapor is responsible for the complex aggregates of colloids formation.

UV-Vis and surface photovoltage spectra of Fe2O3/polystyrene composite microspheres

Fe2O3 sol with the particle diameter of 3-5 nm was flocculated by the addition of SDS, and the flocculate formed was redispersed by the further addition of that surfactant. Thus the surfactant bilayer was formed on the surface of Fe2O3. The emulsion polymerization of styrene (St) adsolubilized oil the surfactant adsorbed bilayer was carried out by initiator potassium persulfate (KPS). The UV-Vis and surface photovoltage spectra (SPS) indicate that the Fe2O3 particles were encapsulated in polystyrene(PSt) successfully.